Abstract
A fast, efficient, and non-chromatographic method was presented in this study for nitrite, nitrate, and p-nitrophenol (N-compounds) extraction and speciation analysis of environmental samples. By applying ultrasound-assisted solid–liquid extraction (USLE), analytes were efficiently extracted from water, soil, or sediment collected in areas of environmental disaster. These analytes were selectively converted to NO(g) through UV photolysis (NO3−), H2O2/UV photocatalysis (PNP), and direct conversion (NO2−). Following conversion, NO(g) was separated from the liquid phase and determined by high-resolution continuum source molecular absorption spectrometry (HR-CS MAS). The LODs obtained were 0.097 ± 0.004 mg L−1 for nitrite, 0.119 ± 0.004 mg L−1 for nitrate, and 0.090 ± 0.006 mg L−1 for p-nitrophenol. On applying this speciation method to environmental samples, concentrations were found to be up to 0.99 ± 0.03 mg L−1 (NO2−), 49.80 ± 2.5 mg L−1 (NO3−), and 0.10 ± 0.02 mg L−1 (PNP). Finally, addition/recovery study of real water, soil, and sediment samples showed 101 ± 2% recovery for NO2−, 100 ± 1% for NO3−, and 96 ± 5% for PNP.
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Funding
This work was financially supported by Fundação de Amparo à Pesquisa do Estado de Minas Gerais (Fapemig), Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES, grant # 88887.368533/2019–00 and Code # 001; 88881.068088/2014–01 and Code # 001), Fundação de Amparo à Pesquisa do Estado de São Paulo (grants: 2013/07296–2, 2014/50249–8, 2017/11986–5), Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), and Shell. J. A.
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All authors contributed to the study conception and design. Ailton José Moreira: writing and Methodology; Carolina Dakuzaku Freschi and Ernesto C. Pereira: writing-review and editing; Gian Paulo Giovanni Freschi: writing, conceptualization, supervision. All authors commented on previous versions of the manuscript. All authors read and approved the final manuscript.
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Highlights
1. Application of a non-chromatographic method for speciation of N-compounds.
2. Fast and efficient extraction of N-compounds in environmental samples of soil and sediments.
3. Effective elimination of matrix interferents during the analytical process.
4. Accessible speciation method for the purpose of environmental monitoring of N-compounds.
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Moreira, A.J., Freschi, C.D., Pereira, E.C. et al. N-compounds speciation analysis in environmental samples using ultrasound-assisted solid–liquid extraction and non-chromatographic techniques. Environ Monit Assess 193, 297 (2021). https://doi.org/10.1007/s10661-021-09088-w
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DOI: https://doi.org/10.1007/s10661-021-09088-w